HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 178448380, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Benzylamine | HCID 7504 | — |
| Reactant | Hexafluorophosphate | HCID 9886 | — |
| Reactant | Boc-D-Valine amide | HCID 10856902 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178448380 | HCID 178448380 | 201.6% |
Reaction Steps
To a stirred solution of Boc-D-Valine amide (10 g, 46 mMol) in CH2Cl2 (200 mL) was added Triethyloxoniuim hexafluorophosphate (13.0 g, 48 mMol). (The reaction started out as a suspension which gradually cleared.) The reaction was stirred for 48 h at RT, poured into a separatory funnel, washed with 1 N Na2CO3, dried (Na2SO4), filtered and concentrated under vacuum. To the remaining oil was added Benzylamine (5.0 mL, 23 mMol) and EtOH (20 mL). The reaction was stirred at 60° C. for 24 h. After cooling to RT the reaction was evaporated under vacuum. The title compound (14.16 g, >95% pure by LCMS) was obtained without purification as a pale yellow oil which eventually solidified to a waxy solid: MS (ES) m/e 306.4 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07166595B2 |
| Source dataset | uspto-grants-2007_01 |
| ORD ID | ord-d17139d7313049e0924f0f0339f69ece |
| Source note | uspto-grants-2007_01 |